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Environ. Sci. Technol.

1992, 26, 772-776

Natural Sorbents in Oil Spill Cleanup


Hyung-Mln Chol"
School of Human Ecology, Louisiana Agricultural Experimental Station, Louisiana State University Agricultural Center,
Baton Rouge, Loulsiana 70803

Rlnn M. Cloud
Department of Clothing and Textiles, Virginia Polytechnic Institute and State University, Blacksburg, Virginia 2406 1

Milkweed (Asclepias) fiber and cotton fiber sorbed


significantly higher amounts of crude oil than polypropylene fiber and polypropylene web from the surface
of an artificial sea water bath containing crude oil and from
a crude oil bath. Milkweed sorbed approximately 40 g of
crude oil/g of fiber at room temperature. The oil sorption
capacity of kenaf core material was comparable with that
of polypropylene web with high-viscosity Bunker C oil.
Only a slight variation was observed in the oil sorption of
the natural fiber sorbent by Soxhlet extraction and
water-soaking treatments before the sorption process.
However, alkali-scouring treatment significantly reduced
the oil sorption capacity of milkweed and cotton fiber. It
was shown that with the aid of suitable mechanical retrieval equipment, sorbed crude oil can be recovered from
milkweed and cotton so the sorbents can be recycled
several times for oil spill cleanup. The results suggested
that a total or partial substitution of commercial synthetic
oil sorbents by natural sorbent materials could be beneficial in the oil spill cleanup operation by improving the
efficiency of oil sorption and by incorporating other advantages such as biodegradability.
Introduction
In March 1989 the Exxon Valdez incident spilled 11.2
million gallons of crude oil into the coastal waters of Prince
William Sound, AK, causing severe environmental damage
(1). The demolition of oil storage tanks in Kuwait during
the war in 1991 spilled several hundred million gallons of
oil into the sea. In addition, oil spills onto land are also
common occurrences even though most spills are usually
small (2).
The presence of sorbent materials in an oil spill area
facilitates a change of phase from liquid to semisolid (3).
Once this change is achieved, the removal of the oil by
removal of the sorbent structure is not difficult. While
hydrophobicity and oleophilicity are primary determinants
of successful sorbents, other important factors include
retention of oil over time, recovery of oil from sorbents,
amount of oil sorbed per unit weight of sorbent, and
reusability and biodegradability of sorbent (2-5).
Oil-sorbent materials can be categorized into three major
classes: inorganic mineral products, organic synthetic
products, and organic vegetable products ( 4 , 5 ) . Mineral
products include perlite, vermiculites, sorbent clay, and
diatomite ( 2 , 5 ) . These materials do not show adequate
buoyancy retention and their oil sorption capacity was
generally low (5). Among synthetic products, polypropylene and polyurethane foam are the most widely used
sorbents in oil spill cleanup because of their highly oleophilic and hydrophobic properties (4, 6). A disadvantage
of these materials is that they degrade very slowly as
compared with mineral or vegetable products. It has been
reported that organic vegetable products such as straw,
corn cob, and wood fiber showed poor buoyancy characteristics, relatively low oil sorption capacity, and low hydrophobicity ( 5 ) .
772

Environ. Scl. Technol., Vol. 26, No. 4, 1992

On the other hand, Johnson et al. (7) later showed the


potential for the utilization of cotton fiber in oil spill
cleanup. More detailed information is needed, however,
before any further application of cotton fiber can be made
in oil spill cleanup. Kobayashi et al. (8)examined a hollow
cellulosic kapok fiber. According to their results, the oil
sorption of kapok fiber used in a mat, block, band, or
screen was approximately 1.5-2.0 times greater than that
of polypropylene mat, which sorbs 11.1g of B-heavy oil
and 7.8 g of machine oil in water.
Milkweed floss (Asclepias),which is cultivated or naturally grown in some states in the United States, is also
a hollow cellulosic material (9). Kenaf is another cellulosic
material readily available in some states. These natural
sorbents have hydrophobic properties before any treatments due to their surface waxes. Milkweed floss, especially, is expected to have high oil sorption capacity because of its high wax content and its hollow structure
similar to kapok. Nevertheless, no work has been reported
on the oil sorption capacity of these materials. If these
natural sorbents show high oil sorption capacity, then they
can be used to substitute non-biodegradable synthetic
materials in oil spill cleanup.
Therefore, the purpose of this research was to study the
oil absorbency of milkweed floss, cotton, and kenaf in a
simulated seawater bath containing crude oil and in a pure
oil bath to examine the feasibility of using these sorbents
in oil spill cleanup.
Experimental Section
Sorbent Materials. Descriptive characteristics of the
sorbents used in this study are given in Table I. The use
of polypropylene materials allowed comparison of natural
fiber sorbents with commonly used sorbent structures.
Natural fibers used in the study had undergone little
processing, thus preserving the natural waxes on the fiber
surfaces, which enhance oleophilicity and hydrophobicity.
To elucidate the effects of these substances, oil sorption
of cotton fibers and milkweed floss was also tested after
solvent extraction and after scouring. Soxhlet extraction
was carried out by the method described in ASTM
D2257-80 (10) using 1,1,2-trichloroethane. Scouring was
done using a solution containing 2% NaOH and 0.5%
Na2C03at pH 13 at boiling temperature.
Since sorbents may encounter water before oil in a spill
cleanup, it is important to know the oil sorption characteristics of water-soaked sorbents. Cotton fiber, milkweed
floss, polypropylene web, and milkweed/polypropylene
web were tested for oil sorption both in the dry state and
after being soaked for 10 min in the artificial seawater.
Crude Oil Samples. The specifications of three crude
oil samples, which were obtained from Placid Refining Co.,
Port Allen, LA, are listed in Table 11. In the early stages
of an oil spill, lighter weight hydrocarbons are evaporated
before any possible cleanup operation can take place (11).
In order to simulate this situation and to minimize experimental variations, crude oil samples were placed in an

0013-936X/92/0926-0772$03.00/0

0 1992 American Chemical Society

Table I. Specifications of Sorbent Materials


fiber types
cotton
milkweed
kenaf
kenaf
polypropylene
milkweed and polypropylene

shape
fiber
fiber
fiber bundle
woody core
fiber
fiber
nonwoven web
nonwoven web

specification

abbreviation

cellulosic fiber
cellulosic fiber
cellulosic fiber
cellulosic material
polypropylene
polypropylene
polypropylene
milkweed (60) polypropylene (40)

COT
MW
KF
KC
PP3
PP15
PPW
MP

fineness
(denier)

length, cm

2.3

2.23
3.0
5-10
0.5-1.0
0.5
47.6

3.0
15.0

Table 11. Specifications of Crude Oil Samples

No. 2 fuel oil (diesel)


light crude oil
No. 6 fuel oil (Bunker C)

w t loss, %

API gravity
(60 OF)

viscos
KIN,,, (100 O F )

spec grav
(60 O F )

after 24 h

after 48 h

35.7
34.2
6.3

3.93
6.46
1024 (122 O F )

0.846
0.854
1.027

6.00
7.50
0.04

6.40
10.50
0.04

efficient hood for 48 h, as described elsewhere (7). The


weight loss of oil samples during the ventilation was considerable for the two low-viscosity crude oils (diesel and
light crude) but not for the high-viscosity oil (Bunker C),
as shown in Table 11. The majority of the weight loss
occurred within 24 h.
Procedure. A 500-mL sample of artificial seawater was
placed in a 1-L glass beaker, as described in AATCC
106-1981(12). The desired amount of oil (10, 20, 30,40,
or 50 g) was added to the beaker. The beaker containing
crude oil and artificial seawater was mounted in a shaking
apparatus (Eberbach Corp.). Approximately 1 g of a
sorbent material was placed in the system, which was
shaken for 10 min at 102 cycles/min. The wetted sorbent
material was weighed after being drained for 1min in the
sustainer. Water content of the sorbent was analyzed by
the distillation technique described in ASTM D95-70 (13).
A mixture of toluene and xylene (20/80, v/v) was used as
the carrier solvent. The amount of oil sorbed by the
sorbent was determined by subtracting the water content
and the initial sorbent weight from the total weight of the
wetted sorbent. The quantity of oil was recorded as grams
per gram of sorbent. For some of the milkweed floss
samples, the bath was prechilled to 5 f 2 "C in the refrigerator and small amounts of ice were added in the bath
during the shaking to keep the temperature constant. At
least two replications were carried out for each sample.
In order to study oil sorption capacity of sorbents
without the water medium, a simple procedure was used.
A 100-mL sample of diesel or light crude oil was placed
in a 200-mL beaker before any sorbent was immersed in
the bath. After shaking and draining as described above,
the amounts of oil sorbed by the sorbent were determined
by a gravimetric method.
Recovery of Sorbed Oil and Reusability of Sorbents. Another set of specimens was tested to determine
recovery of oil sorbed in the sorbent and reusability of
sorbents. With 40 g of light crude oil in the artificial
seawater bath, the same sorption procedure was used, but
water content was determined by evaporation in the hood,
as described in the previous study (7), rather than by
solvent distillatmionsince the latter procedure would affect
subsequent oil sorption of materials. This method gives
an approximate oil sorption value. The sorbent with oil
was squeezed between two rollers at 344.5 X lo3Pa (50 psi)
before it was reweighed to determine the amount of recovered oil. The squeezed sorbent was again used in the
sorption process. The efficiency of sorbent reusability was

ca,

50,

40m

a
v
+-

30-

a,

20-

w
a,

5
.--c
.0

10-

0
0

10

20

30

40

50

60

Oil in the artificial sea water(g/500rnl)


Flgure 1. Light crude oil sorption. Key: 0, COT; B, PPW; @, MW;
V, KF; A, PP3; V, KC; A, PP15; 0 ,MW (at 5 "C); 0,MP.

a"

30

I2ol
a,

5
.-

'E

10

l
10

20

j
30

40

l
50

60

Oil in the artificial sea water(g/500rnl)


Figure 2. Bunker C oil sorption. Key: 0, COT; @, MW; A, PP15; B,
PPW; 7 , KC.

determined by oil sorption capacity of each sorbent after


repeated sorption and desorption cycles.
Results-and Discussion
Sorption from Artificial Seawater. The oil sorption
characteristics of different sorbents in the artificial seawater baths containing different amounts of oil are shown
in Figures 1 and 2 for light crude oil and Bunker C oil,
respectively. Even though it is not shown here, sorption
trends of the sorbents with diesel oil are very similar to
those of light crude oil due to the similar specific gravities
of both oil samples. According to Johnson's results (8,
Environ. Sci. Technol., Vol. 26, No. 4, 1992

773

oil sorbed on cotton increased with increasing specific


gravity until it reached unity and then decreased. However, they did not explain why this phenomenon occurred.
The specific gravity of Bunker C employed in this study
was even higher than unity. Because of this high specific
gravity, some portion of Bunker C oil, which was sunken
in the seawater bath, made minimum contact with the
sorbent during the sorption process. This contributed to
the low sorption capacity of sorbents with Bunker C oil,
with the exception of polypropylene fiber.
Among the sorbent materials examined in this research,
milkweed floss showed the highest oil sorption capacity,
followed by cotton fiber. One gram of milkweed floss can
sorb -40 g of light crude oil at room temperature. Unfortunately, the exact fineness of the fiber is not known,
but observation by a light microscope revealed that milkweed fiber was coarser than cotton. The milkweed ranged
in diameter from 20 to 50 pm while American upland
cotton was approximately 25 pm (14). Therefore, the exceptionally high oil sorption by milkweed fiber can be
explained by the large amount of wax on the fiber surface,
-3% compared with the 0 . 4 4 8 % wax content of cotton,
and the larger and noncollapsing lumen of the fiber, which
gives more void volume for absorbed oil. The wall thickness of milkweed is only 10% of the total diameter of the
fiber (9).
The oil sorption of milkweed was increased at 5 f 2 "C,
as shown in Figure 1. Increase of oil sorption at a low
temperature was also observed in another study with other
sorbents, which suggested that this increase was due to an
increase in oil viscosity at this temperature (7). However,
Schatzberg (5) pointed out that the rate of oil penetration
into a capillary is inversely proportional to the oil viscosity
and directly proportional to the capillary radius. It was
also expected that a decrease in temperature should decrease the segmental mobility of the fiber, which would
reduce the rate of absorption. At the initial stage of adsorption of oil onto the fiber surface, some interactions
such as hydrophobic interaction and van der Waals force
would occur between crude oil in the bath and wax in the
natural sorbents. However, the absorption of oil within
the fiber could be mainly influenced by the diffusion of
oil through internal capillary movement, particularly for
milkweed and cotton due to their lumens. Therefore, an
increase in oil viscosity reduces the rate of absorption
within the internal capillary movement of oil, but at same
time it increases the adherence of oil onto the surface of
the fiber and within the capillary during drainage. The
experimental results of increase of oil sorption capacity
with decrease in temperature, subsequently, and with increase in oil viscosity, implied that sorption time (10 min)
was sufficient to minimize the effect of rate of absorption
on oil sorption capacity of the sorbent. Extension of the
sorption time to 30 and 60 min resulted in practically equal
values in the oil sorption of milkweed floss. It was pointed
out (5) that the oil sorption rates were very rapid so that
the maximum capacity was nearly attained for most sorbents in 5 min. Furthermore, the results also suggested
that at 5 f 2 "C the decrease in segmental mobility of the
fiber probably was not a significant effect in this case.
In comparison, 1 g of polypropylene fiber or polypropylene web only sorbed approximately 10 g of light
crude oil, As expected, polypropylene fiber initially attracted large amounts of oil from the surface of the system
because of its oleophilicity, but during the drainage, the
fiber wad did not hold oil well so that large amounts of
excess oil were drained. This phenomenon appeared to
be more significant in light crude oil due to its low vis774

Environ. Sci. Technol., Vol. 26, No. 4, 1992

Figure 3. Oil sorption of water-soaked sorbents in the artificial seawater bath containing 10 and 40 g of light crude oil. Key: 0,regular
(40 g of oil); a, water soaked (40 g of oil): El, regular (10 g of oil): ,.
water soaked (10 g of oil).

cosity. Unlike other sorbent materials, the oil sorption


capacity of polypropylene fiber (15 denier) was increased
with Bunker C oil. Zahid et al. (15)claimed that the main
mechanism in the oil sorption of polypropylene fiber was
capillary bridges in the voids between the fibers rather
than absorption or adsorption due to its high crystallinity.
In this case, high viscous Bunker C would form a very
coherent mass with polypropylene fiber so its oil sorption
capacity should be increased. The fiber denier of the
polypropylene fiber was considered one of factors in determining its oil sorption capacity (7). However, in the
present study this effect was not clearly shown (Figure l),
presumably due to the considerable difference in crimping.
The reduction in surface area with increase in fiber denier
was compensated for by the effect of crimping, which, as
described in the previous work (7), increased the accessible
fiber surface area and, consequently, increased the oil
sorption. In addition, since the staple length of 3-denier
polypropylene fiber was extremely short, the geometry of
the fiber wad was probably not favorable for oil adherence
between fibers.
The nonwoven web made 60% milkweed with 40%
polypropylene fiber resulted in oil sorption midway between the values obtained by milkweed floss and polypropylene web. Often sorbents are structured into sheets,
booms, or pads, which are reusable and easier to control.
In addition, the collection ability of these materials after
application in an oil spill cleanup should be increased by
making such structures. Since the introduction of milkweed in the web considerably increased the oil sorption
capacity of polypropylene pad, the blending percentage
should be further optimized in terms of their performance
characteristics.
The oil sorption capacity of cotton fiber was lower than
milkweed floss but still approximately 2.5-3 times higher
than polypropylene web or fibers. Therefore, this study
confirmed the previous result suggesting cotton fibers as
potential sorbents for oil spill cleanup.
The oil sorption values of kenaf fiber and core materials
were generally lower than that of milkweed or cotton but
were similar to polypropylene web for heavy Bunker C oil.
Kenaf fiber is much coarser than cotton and milkweed, and
it occurs in a fiber bundle rather than a single fiber.
Further separation of this fiber bundle to the single fibers
should increase oil sorption comparably to polypropylene.
As seen in Figure 3, the presoaking of sorbent by water
only slightly modified the oil sorption characteristics of
sorbent materials with both 10 and 40 g of light crude oil
in the bath. Since cotton, milkweed, and polypropylene
are hydrophobic in nature, the water sorption during 10
min of soaking time was minimal.

Table 111. Recovery of Oil and Reusability of Sorbents after Squeezing by Two Rollersa
fiber

oil sorbed

COT
MW

33.2
38.5
26.8
11.3

MP

PPW

first cycle
oil remainingb

second cycle
oil sorbed"
oil remainingb
with Light Crude Oild
27.9 (84)
35.0 (91)
24.6 (92)
9.4 (83)

1.5 (95)
1.2 (97)
1.8 (93)
1.7 (85)

1.3 (95)
1.3 (96)
1.7 (93)
1.6 (83)

oil sorbed'

third cycle
oil remaining'
1.2 (95)
1.4 (96)
1.7 (93)
1.6 (83)

24.5 (74)
32.9 (85)
24.1 (90)
9.4 (83)

'

Units are gram of oil per gram of sorbent. Values in parentheses represent percentage of recovered oil from the sorbent against the
amount of oil sorbed in each cycle. Values in parentheses represent percentage of sorbed oil against amount of oil sorbed in the first cycle.
dAmount, 40 g/500 mL of artificial seawater.
60

1 untreated
2 extracted

COT

UW

PPW

MP

PP3

PP15

Flgure 4. Oil sorption in the oil bath. Key: 0 ,light crude; H,NO. 2
fuel; H, No. 2 fuel extracted; H, No 2 fuel scoured.

Sorption without Water Medium. Often the sorbents


are used to clean oil in the areas in which no water is
involved, Since the sorption environment is different, oil
sorption of sorbents is expected to be changed. In addition,
this method would determine the maximum amount of oil
sorbed by a particular sorbent. Figure 4 shows that oil
sorption by the sorbent in the oil bath was slightly higher
than the oil sorption in the artificial seawater bath containing 40 or EiO g of oil. The sorption of light crude oil
by the sorbent was generally slightly higher than the
sorption of diesel oil. Again, cotton and milkweed had
considerable higher oil sorption capacities than polypropylene web and fiber. The nonwoven web of milkweed
and polypropylene showed higher oil sorption than polypropylene web and fiber but lower sorption than cotton
and milkweed. Therefore, it can be concluded that these
natural sorbent materials should be suitable to remove oil
not only from the surface of seawater, but also from places
in which no water is involved.
Extracted rind Scoured Sorbents. The Soxhlet extraction of cotton and milkweed fibers with 1,1,2-trichloroethane did not reduce their oil sorption capacities
in diesel and light crude oil bath without artificial seawater
(Figure 4) or in the artificial seawater bath containing 40
g of diesel oil (Figure 5). In the previous work (8,
cotton
fiber was extracted by a similar organic solvent (trichloroethylene), and there was only a marginal decrease
in oil sorption capacity. It was not clear why the extracted
fibers sorbed such high amounts of oil. According to
Derry's result (16),immersion in trichloroethylene for 30
s reduced the wax content of an Indian grey cotton cloth
from 1.09 to 0.15%. Therefore, it may be unreasonable
to suspect the efficiency of Soxhlet extraction in removing
surface waxes. A plausible explanation is that the fiber
remained oleophilic due to residual organic solvents.
On the other hand, alkali-scouring treatment of cotton
and milkweed significantly decreased their oil sorption
capacities both in the pure oil bath (Figure 4) and in the
artificial seawater bath containing oil (Figure 5). Both

MW
Flgure 5. Oil sorption of extracted and scoured sorbents in the artificial
seawater bath containing 40 g of diesel oil. Key: 0,oil; H, water.

milkweed and cotton sorbed less than 10 g of diesel oil from


an artificial seawater bath containing 40 g of diesel oil. As
expected, water sorption by cotton was increased more
than 10 times due to the removal of the natural wax
coating making the fiber more hydrophilic. Alkali scouring
of milkweed produced a hard, pulplike product, which
resulted in less sorption of oil and water. However, even
after the scouring treatment, cotton and milkweed sorbed
18.4 and 8.7 g of diesel oil from the pure oil bath, respectively, which is still comparable with values obtained
for the polypropylene fiber.
Recovery of Oil and Reusability of Sorbents. Although more efficient means of recovering oil from the
sorbent are available, compression of the sorbent is an
economical and practical method. More than 90% of the
sorbed oil was removed from the sorbents by a simple
mechanical action, as given in Table 111. The recovery
of oil was decreased to 7945% for the polypropylene web,
suggesting stronger interactions between oil and polypropylene. If the contamination of the recovered oil is low,
it can be recycled.
The sorbent is considered reusable if a loaded sorbent
can be easily compressed or squeezed to its original size
and shape (2). Even if there was a tendency toward decrease in sorbent efficiency with the repeated sorption and
desorption, in the third sorption, milkweed and cotton
fibers sorbed approximately 74-85% of the oil sorbed in
the first sorption. For web samples, the oil sorption capacity tended to be slightly higher than fiber samples.
These results suggest that, like polypropylene sorbent,
cotton and milkweed sorbents can be recycled several times
for oil spill cleanup with the aid of a suitable mechanical
device.
Conclusion
We examined the oil sorption capacities of three natural
fiber sorbents, milkweed, cotton, and kenaf, to determine
their potential use in oil spill cleanup. Milkweed showed
Environ. Sci. Technol., Vol. 26, No, 4, 1992 775

the highest oil sorption capacity followed by cotton fiber.


The high oil sorption capacity of milkweed fiber was due
to the large amount of wax on the fiber surface and the
larger and noncollapsing lumen of the fiber. Both milkweed and cotton sorbed larger amounts of crude oil than
polypropylene fiber and polypropylene web, which are
commercially used as sorbents in oil spill cleanup. In
general, the sorbents sorbed less of the heavy Bunker C
oil than the other oil samples, with the exception of polypropylene fiber.
Solvent extraction and presoaking in water only slightly
modified the oil sorption characteristics of the sorbents.
On the other hand, an alkali-scouring treatment significantly reduced the oil sorption ability of the natural fiber
sorbents. The majority of the sorbed oil was removed from
the natural sorbents by a simple mechanical action, suggesting that the sorbents can be used repeatedly in oil spill
cleanup.
The results suggested that a total or partial substitution
of commercial synthetic oil sorbents, such as polypropylene, by natural sorbent materials, such as milkweed
and cotton, could be beneficial in the oil spill cleanup
operation by improving the efficiency of oil sorption and
by incorporating other advantages such as biodegradability.

Acknowledgments
We acknowledge Placid Refining Co., Natural Fibers
Corp., Hercules, Inc., 3M, and H. Willett & Associates for
supplying crude oil samples, milkweed floss, polypropylene
fibers, polypropylene webs, and kenaf, respectively.
Thanks also go to Y. Chen for laboratory assistance and
G. Simmons for preparing the manuscript.

Literature Cited
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196-200.
(2) Melvold, R. W.; Gibson, S. C.; Scarberry, R. Sorbents for
Liquid Hazardous Substance Cleanup and Control; Noyes

776

Environ. Scl. Technol., Vol. 26, No. 4, 1992

Data Corp.: Park Ridge, NJ, 1988.


(3) Halligan, J. E.; Ball, A. A.; Meenaghan, G. F. U.S. Coast
Guard Report No. CG-D-63-76; U.S. Coast Guard Headquarters, Washington, DC, 1976.
(4) T h e International Tanker Owner Pollution Federation
Limited. Measures to Combat Oil Pollution; Graham &
Trotman Limited: London, 1980.
(5) Schatzberg, P. U.S.
Coast Guard Report No. 724110.1/2/1;
U.S. Coast Guard Headquarters, Washington, DC, 1971.
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Sci. Technol. 1973, 7, 439-443.
( 8 ) Kobayashi, Y.; Matsuo, R.; Nishiyama, M. Japanese Patent
52,138,081, November 17, 1977.
(9) Knudsen, H. D. Presented in TAPPI Nonwovens Conference, May 6-10, 1990, Marco Islands, FL, Technical Association of the Pulp and Paper Industry.
(10) ASTM D2257-80. Annual Book of A S T M Standards;
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PA, 1990; Vol. 07.01.
(11) Galt, J. A,; Lehr, W. J.; Paytan, D. L. Enuiron. Sci. Technol.
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(12) AATCC 106-1981. Technical Manual of the American
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(13) ASTM D95-70. Annual Book of A S T M Standards; American Society of Testing and Materials: Philadelphia, PA,
1971; Part 17.
(14) Bailey, T. L. W., Jr. In Mattews Textile Fibers; Mauersberger, H. R., Ed.; John Wiley & Sons, Inc.: New York,
1954; Chapter IV, pp 172-173. Whitford, A. C. Ibid.
Chapter IX, pp 450-452.
(15) Zahid, M. A.; Halligan, J. E.; Johnson, J. E. Ind. Erg. Chem.,
Proc. Res. Dev. 1972, 11, 550-555.
(16) Derry, R. L. J. SOC.Dyers Colour. 1955, 71, 884-893.

Received for review August 14,1991. Revised manuscript received


December 16, 1991. Accepted December 18, 1991.

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